#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:48:28 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178793 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/47/4104794.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4104794
loop_
_publ_author_name
'Madhab C. Das'
'Parimal K. Bharadwaj'
_publ_section_title
;
 A Porous Coordination Polymer Exhibiting Reversible Single-Crystal to
 Single-Crystal Substitution Reactions at Mn(II) Centers by Nitrile Guest
 Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10942
_journal_page_last               10949
_journal_paper_doi               10.1021/ja9006035
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C38 H35 Mn2 N9 O8'
_chemical_formula_weight         855.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.510(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.777(7)
_cell_length_b                   15.303(5)
_cell_length_c                   16.267(6)
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.5
_cell_volume                     4058(3)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12847
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.8985
_exptl_absorpt_correction_T_min  0.8811
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABAS 2.10 (Bruker 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4918
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.2191
_reflns_number_gt                3670
_reflns_number_total             4918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9006035_si_002_02.cif
_cod_data_source_block           complex2
_cod_database_code               4104794
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mn1 Mn 0.26745(9) 0.11011(9) 0.54514(9) 0.0237(7) Uani 1 1 d .
O1 O 0.2782(5) 0.0266(4) 0.6624(5) 0.0308(16) Uani 1 1 d .
O2 O 0.2514(5) -0.0397(5) 0.5335(5) 0.0321(17) Uani 1 1 d .
O4 O 0.2997(5) 0.2315(4) 0.6082(5) 0.0289(16) Uani 1 1 d .
O3 O 0.2437(5) 0.1299(4) 0.4092(5) 0.0297(17) Uani 1 1 d .
N2 N 0.1874(6) -0.3530(6) 0.5840(6) 0.036(2) Uani 1 1 d .
H2 H 0.1961 -0.3540 0.5357 0.089 Uiso 1 1 calc R
C1 C 0.2415(7) -0.1238(7) 0.7371(7) 0.029(2) Uani 1 1 d .
H1 H 0.2545 -0.0729 0.7711 0.035 Uiso 1 1 calc R
C6 C 0.2777(6) 0.3003(6) 0.7280(6) 0.025(2) Uani 1 1 d .
C8 C 0.2582(6) -0.0408(6) 0.6141(6) 0.027(2) Uani 1 1 d .
C4 C 0.2048(6) -0.2782(6) 0.6345(7) 0.0245(19) Uani 1 1 d .
N1 N 0.4013(6) 0.0921(6) 0.5682(6) 0.0299(19) Uani 1 1 d .
C2 C 0.2412(6) -0.1241(6) 0.6522(7) 0.025(2) Uani 1 1 d .
N4 N 0.1343(7) 0.1239(7) 0.5205(9) 0.038(3) Uani 1 1 d D
C5 C 0.2971(6) 0.2233(6) 0.7788(6) 0.0240(19) Uani 1 1 d .
H5 H 0.3113 0.1731 0.7560 0.059 Uiso 1 1 calc R
C3 C 0.2223(6) -0.1999(7) 0.6009(7) 0.028(2) Uani 1 1 d .
H3 H 0.2212 -0.1987 0.5432 0.063 Uiso 1 1 calc R
C7 C 0.2784(6) 0.2993(6) 0.6358(6) 0.0236(19) Uani 1 1 d .
C11 C 0.5663(7) 0.0788(7) 0.5952(7) 0.032(2) Uani 1 1 d .
C14 C 0.1552(7) -0.4294(6) 0.6091(7) 0.035(2) Uani 1 1 d .
H14A H 0.1877 -0.4418 0.6718 0.058 Uiso 1 1 calc R
H14B H 0.1609 -0.4786 0.5744 0.058 Uiso 1 1 calc R
C10 C 0.5156(7) 0.1416(8) 0.5393(9) 0.042(3) Uani 1 1 d .
H10 H 0.5359 0.1806 0.5092 0.051 Uiso 1 1 calc R
C12 C 0.5315(7) 0.0222(8) 0.6367(8) 0.039(3) Uani 1 1 d .
H12 H 0.5633 -0.0211 0.6748 0.047 Uiso 1 1 calc R
C15 C 0.0642(15) 0.1095(13) 0.490(2) 0.042(8) Uani 1 1 d D
C13 C 0.4510(8) 0.0301(8) 0.6217(8) 0.042(3) Uani 1 1 d .
H13 H 0.4290 -0.0092 0.6497 0.051 Uiso 1 1 calc R
C9 C 0.4340(8) 0.1460(8) 0.5284(9) 0.044(3) Uani 1 1 d .
H9 H 0.4008 0.1891 0.4912 0.053 Uiso 1 1 calc R
C18 C 0.0000 0.2676(15) 0.2500 0.061(6) Uani 1 2 d S.
H18A H -0.0334 0.2885 0.1910 0.072 Uiso 0.50 1 calc PR
H18B H 0.0551 0.2885 0.2672 0.072 Uiso 0.50 1 calc PR
H18C H -0.0217 0.2885 0.2918 0.072 Uiso 0.50 1 calc PR
C17 C 0.0000 0.1701(16) 0.2500 0.062(3) Uani 1 2 d SD
N3 N 0.0000 0.096(2) 0.2500 0.033(13) Uani 1 2 d SD
C16 C -0.0284(16) 0.106(3) 0.453(3) 0.052(2) Uani 1 1 d .
H16A H -0.0454 0.0563 0.4771 0.083 Uiso 1 1 calc R
H16B H -0.0495 0.1012 0.3888 0.083 Uiso 1 1 calc R
H16C H -0.0490 0.1585 0.4690 0.083 Uiso 1 1 calc R
C19 C -0.1092(18) -0.077(2) 0.257(3) 0.066(2) Uani 1 1 d D
C20 C -0.122(2) -0.064(4) 0.161(2) 0.065(2) Uani 1 1 d .
H20A H -0.1023 -0.0076 0.1540 0.084 Uiso 1 1 calc R
H20B H -0.1790 -0.0693 0.1235 0.084 Uiso 1 1 calc R
H20C H -0.0916 -0.1083 0.1447 0.084 Uiso 1 1 calc R
N5 N -0.097(7) -0.088(4) 0.328(3) 0.050(11) Uani 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Mn1 O3 106.8(3) . .
O4 Mn1 O1 100.1(3) . .
O3 Mn1 O1 153.1(3) . .
O4 Mn1 N4 93.9(4) . .
O3 Mn1 N4 92.5(4) . .
O1 Mn1 N4 86.1(3) . .
O4 Mn1 N1 87.8(3) . .
O3 Mn1 N1 87.1(3) . .
O1 Mn1 N1 93.5(3) . .
N4 Mn1 N1 178.3(4) . .
O4 Mn1 O2 157.5(3) . .
O3 Mn1 O2 95.2(3) . .
O1 Mn1 O2 57.9(2) . .
N4 Mn1 O2 89.5(4) . .
N1 Mn1 O2 88.9(3) . .
O4 Mn1 C8 129.0(3) . .
O3 Mn1 C8 124.2(3) . .
O1 Mn1 C8 28.9(3) . .
N4 Mn1 C8 85.2(4) . .
N1 Mn1 C8 93.6(3) . .
O2 Mn1 C8 29.2(3) . .
C8 O1 Mn1 91.7(6) . .
C8 O2 Mn1 88.3(6) . .
C7 O4 Mn1 148.5(7) . .
C7 O3 Mn1 127.8(6) 7_556 .
C4 N2 C14 122.1(9) . .
C4 N2 H2 118.9 . .
C14 N2 H2 119.0 . .
C2 C1 C6 120.1(9) . 4_546
C2 C1 H1 119.9 . .
C6 C1 H1 120.0 4_546 .
C1 C6 C5 120.3(9) 4_556 .
C1 C6 C7 121.0(9) 4_556 .
C5 C6 C7 118.7(8) . .
O1 C8 O2 121.4(9) . .
O1 C8 C2 119.5(8) . .
O2 C8 C2 119.0(9) . .
O1 C8 Mn1 59.4(5) . .
O2 C8 Mn1 62.5(5) . .
C2 C8 Mn1 172.2(7) . .
N2 C4 C3 120.8(9) . .
N2 C4 C5 121.2(8) . 4_546
C3 C4 C5 118.0(8) . 4_546
C9 N1 C13 116.9(10) . .
C9 N1 Mn1 118.7(7) . .
C13 N1 Mn1 124.3(8) . .
C1 C2 C3 120.5(9) . .
C1 C2 C8 119.3(9) . .
C3 C2 C8 120.2(9) . .
C15 N4 Mn1 158.9(16) . .
C6 C5 C4 119.9(8) . 4_556
C6 C5 H5 120.0 . .
C4 C5 H5 120.0 4_556 .
C2 C3 C4 121.1(9) . .
C2 C3 H3 119.4 . .
C4 C3 H3 119.4 . .
O4 C7 O3 124.4(9) . 7_556
O4 C7 C6 119.5(8) . .
O3 C7 C6 116.2(8) 7_556 .
C10 C11 C12 117.0(10) . .
C10 C11 C14 121.7(10) . 3
C12 C11 C14 121.2(10) . 3
N2 C14 C11 113.7(9) . 3_445
N2 C14 H14A 108.8 . .
C11 C14 H14A 108.8 3_445 .
N2 C14 H14B 108.8 . .
C11 C14 H14B 108.8 3_445 .
H14A C14 H14B 107.7 . .
C11 C10 C9 119.4(10) . .
C11 C10 H10 120.3 . .
C9 C10 H10 120.3 . .
C13 C12 C11 120.0(11) . .
C13 C12 H12 120.0 . .
C11 C12 H12 119.9 . .
N4 C15 C16 171(2) . .
N1 C13 C12 123.3(11) . .
N1 C13 H13 118.4 . .
C12 C13 H13 118.3 . .
N1 C9 C10 123.3(10) . .
N1 C9 H9 118.4 . .
C10 C9 H9 118.3 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N3 C17 C18 180.000(5) . .
C15 C16 H16B 109.6 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.9 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N5 C19 C20 177(6) . .
C19 C20 H20A 108.1 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.0 . .
H20A C20 H20C 109.4 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 2.089(7) .
Mn1 O3 2.100(7) .
Mn1 O1 2.240(7) .
Mn1 N4 2.247(11) .
Mn1 N1 2.273(10) .
Mn1 O2 2.310(7) .
Mn1 C8 2.601(10) .
O1 C8 1.259(12) .
O2 C8 1.268(11) .
O4 C7 1.249(12) .
O3 C7 1.278(12) 7_556
N2 C4 1.370(12) .
N2 C14 1.431(13) .
N2 H2 0.8600 .
C1 C2 1.379(15) .
C1 C6 1.393(13) 4_546
C1 H1 0.9300 .
C6 C1 1.393(13) 4_556
C6 C5 1.402(13) .
C6 C7 1.505(12) .
C8 C2 1.499(13) .
C4 C3 1.403(13) .
C4 C5 1.424(13) 4_546
N1 C9 1.318(15) .
N1 C13 1.351(14) .
C2 C3 1.390(14) .
N4 C15 1.16(3) .
C5 C4 1.424(13) 4_556
C5 H5 0.9300 .
C3 H3 0.9300 .
C7 O3 1.278(12) 7_556
C11 C10 1.381(16) .
C11 C12 1.386(16) .
C11 C14 1.510(16) 3
C14 C11 1.510(16) 3_445
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C10 C9 1.392(18) .
C10 H10 0.9300 .
C12 C13 1.358(17) .
C12 H12 0.9300 .
C15 C16 1.51(3) .
C13 H13 0.9300 .
C9 H9 0.9300 .
C18 C17 1.491(14) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C17 N3 1.13(3) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C19 N5 1.10(7) .
C19 C20 1.50(5) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9601 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O4 Mn1 O1 C8 -179.6(6) . .
O3 Mn1 O1 C8 -0.6(10) . .
N4 Mn1 O1 C8 87.2(7) . .
N1 Mn1 O1 C8 -91.1(6) . .
O2 Mn1 O1 C8 -4.7(6) . .
O4 Mn1 O2 C8 17.9(11) . .
O3 Mn1 O2 C8 -173.5(6) . .
O1 Mn1 O2 C8 4.6(6) . .
N4 Mn1 O2 C8 -81.1(7) . .
N1 Mn1 O2 C8 99.5(6) . .
O3 Mn1 O4 C7 95.7(13) . .
O1 Mn1 O4 C7 -84.7(13) . .
N4 Mn1 O4 C7 2.0(13) . .
N1 Mn1 O4 C7 -177.9(13) . .
O2 Mn1 O4 C7 -96.1(14) . .
C8 Mn1 O4 C7 -85.0(13) . .
O4 Mn1 O3 C7 -24.7(9) . 7_556
O1 Mn1 O3 C7 156.4(8) . 7_556
N4 Mn1 O3 C7 70.1(9) . 7_556
N1 Mn1 O3 C7 -111.5(8) . 7_556
O2 Mn1 O3 C7 159.9(8) . 7_556
C8 Mn1 O3 C7 156.0(8) . 7_556
Mn1 O1 C8 O2 8.5(10) . .
Mn1 O1 C8 C2 -171.1(8) . .
Mn1 O2 C8 O1 -8.2(10) . .
Mn1 O2 C8 C2 171.3(8) . .
O4 Mn1 C8 O1 0.5(8) . .
O3 Mn1 C8 O1 179.7(6) . .
N4 Mn1 C8 O1 -90.6(7) . .
N1 Mn1 C8 O1 90.7(6) . .
O2 Mn1 C8 O1 171.8(10) . .
O4 Mn1 C8 O2 -171.3(5) . .
O3 Mn1 C8 O2 7.8(7) . .
O1 Mn1 C8 O2 -171.8(10) . .
N4 Mn1 C8 O2 97.6(7) . .
N1 Mn1 C8 O2 -81.1(6) . .
C14 N2 C4 C3 -168.6(10) . .
C14 N2 C4 C5 9.1(15) . 4_546
O4 Mn1 N1 C9 -63.9(9) . .
O3 Mn1 N1 C9 43.0(9) . .
O1 Mn1 N1 C9 -163.9(9) . .
O2 Mn1 N1 C9 138.3(9) . .
C8 Mn1 N1 C9 167.1(9) . .
O4 Mn1 N1 C13 115.0(9) . .
O3 Mn1 N1 C13 -138.0(9) . .
O1 Mn1 N1 C13 15.0(9) . .
O2 Mn1 N1 C13 -42.8(9) . .
C8 Mn1 N1 C13 -14.0(9) . .
C6 C1 C2 C3 -0.3(16) 4_546 .
C6 C1 C2 C8 177.1(10) 4_546 .
O1 C8 C2 C1 5.2(15) . .
O2 C8 C2 C1 -174.4(10) . .
O1 C8 C2 C3 -177.4(10) . .
O2 C8 C2 C3 3.1(15) . .
O4 Mn1 N4 C15 166(4) . .
O3 Mn1 N4 C15 59(4) . .
O1 Mn1 N4 C15 -94(4) . .
O2 Mn1 N4 C15 -36(4) . .
C8 Mn1 N4 C15 -65(4) . .
C1 C6 C5 C4 1.7(15) 4_556 4_556
C7 C6 C5 C4 -178.6(8) . 4_556
C1 C2 C3 C4 -1.4(16) . .
C8 C2 C3 C4 -178.9(9) . .
N2 C4 C3 C2 -179.0(9) . .
C5 C4 C3 C2 3.2(15) 4_546 .
Mn1 O4 C7 O3 -93.8(14) . 7_556
Mn1 O4 C7 C6 86.1(14) . .
C1 C6 C7 O4 176.5(10) 4_556 .
C5 C6 C7 O4 -3.2(14) . .
C1 C6 C7 O3 -3.6(14) 4_556 7_556
C5 C6 C7 O3 176.7(9) . 7_556
C4 N2 C14 C11 73.4(13) . 3_445
C12 C11 C10 C9 0.9(18) . .
C14 C11 C10 C9 179.6(11) 3 .
C10 C11 C12 C13 -0.1(17) . .
C14 C11 C12 C13 -178.8(11) 3 .
C9 N1 C13 C12 1.0(18) . .
Mn1 N1 C13 C12 -177.9(9) . .
C11 C12 C13 N1 -0.9(19) . .
C13 N1 C9 C10 -0.2(19) . .
Mn1 N1 C9 C10 178.8(10) . .
C11 C10 C9 N1 -1(2) . .
